Methyl iodide → HCID 12263408、化合物
反応式
[CH3:1][C:2]1[N:3]=[C:4]([NH:10][CH3:11])[S:5][C:6]=1[C:7](=[O:9])[CH3:8].[H-].[Na+].[CH3:14]I>C1COCC1.CCOC(C)=O>[CH3:11][N:10]([CH3:14])[C:4]1[S:5][C:6]([C:7](=[O:9])[CH3:8])=[C:2]([CH3:1])[N:3]=1参加物
6
実験手順
A mixture of 1-(4-methyl-2-methylamino-thiazol-5-yl)-ethanone (0.40 g, 2.4 mmol) in THF (2 mL) was treated with NaH (0.113 g, 4.7 mmol). After heating at 40° C. for 0.5 h MeI (0.35 g, 2.4 mmol) was added. Heating was continued for a further 2 h. After cooling, the solution was diluted with EtOAc, washed with brine, and dried over MgSO4. The solvent was evaporated to afford 1-(2-dimethylamino-4-methyl-thiazol-5-yl)-ethanone as a yellow solid. 1H-NMR (CDCl3) δ: 2.36 (s, 3H, CH3), 2.51 (s, 3H, CH3), 3.10 (s, 6H, CH3).
後処理
- additionwas added
- temperatureHeating
- temperatureAfter cooling
- washwashed with brine
- dry with materialdried over MgSO4
- customThe solvent was evaporated
出典と根拠
- ORDレコード
- ord-75556bd194b34770aedfa394501cf480
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07427627B2
反応ノート
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